A phosphorus-sulfur co-doped graphene supported mo 2 c Composite material preparation method

A composite material and co-doping technology, which is applied in the field of preparation of phosphorus-sulfur co-doped graphene-loaded Mo2C composite materials, can solve the problems of consuming large fossil energy and achieve improved catalytic activity and stability, good electrocatalytic performance, The effect of increasing the specific surface area

Active Publication Date: 2022-05-06
北京时代思动科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The reaction process requires pure H 2 As a reactant and under high temperature and high pressure environment, it will consume a lot of fossil energy

Method used

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  • A phosphorus-sulfur co-doped graphene supported mo <sub>2</sub> c Composite material preparation method
  • A phosphorus-sulfur co-doped graphene supported mo <sub>2</sub> c Composite material preparation method
  • A phosphorus-sulfur co-doped graphene supported mo <sub>2</sub> c Composite material preparation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] A phosphorus-sulfur co-doped graphene supported Mo 2 C composite material, preparation method comprises the following steps:

[0024] (1) Add 100mg graphene oxide into 150ml deionized water, ultrasonically disperse for 1h, add 150μl phosphoric acid, ultrasonically mix for 8h until uniform, then pour the mixed sample into a watch glass, dry at 85°C for 12h, and then transfer to a muffle furnace In the process, the temperature was raised to 800°C at a rate of 5°C / min, and calcined for 3h;

[0025] (2) Add the product of step (1) into 200ml of deionized water, ultrasonically disperse for 1h, add 150μl of sulfuric acid, ultrasonically mix for 2h until uniform, freeze-dry, then heat up to 1000°C at a rate of 5°C / min, and calcined for 2h to obtain Phosphorus and sulfur co-doped graphene supported Mo 2 C material.

[0026] (3) Add the product of step (2) into deionized water, ultrasonicate for 45min, add 300mg of ammonium molybdate tetrahydrate into 20ml of deionized water,...

Embodiment 2

[0028] A phosphorus-sulfur co-doped graphene supported Mo 2 C composite material, preparation method comprises the following steps:

[0029] (1) Add 100mg graphene oxide to 150ml deionized water, ultrasonically disperse for 1h, add 100μl phosphoric acid, ultrasonically mix for 8h until uniform, then pour the mixed sample into a watch glass, dry at 85°C for 12h, and then transfer to a muffle furnace In the process, the temperature was raised to 700°C at a rate of 2°C / min, and calcined for 2h;

[0030] (2) Add the product of step (1) into 200ml of deionized water, ultrasonically disperse for 1h, add 100μl of sulfuric acid, ultrasonically mix for 2h until uniform, freeze-dry, then heat up to 800°C at a rate of 2°C / min, and calcined for 1h to obtain Phosphorus and sulfur co-doped graphene supported Mo 2 C material.

[0031] (3) Add the product of step (2) into deionized water, ultrasonicate for 30min, add 200mg of ammonium molybdate tetrahydrate into 20ml of deionized water, st...

Embodiment 3

[0033] A phosphorus-sulfur co-doped graphene supported Mo 2 C composite material, preparation method comprises the following steps:

[0034] (1) Add 100mg graphene oxide into 150ml deionized water, ultrasonically disperse for 1h, add 150μl phosphoric acid, ultrasonically mix for 8h until uniform, then pour the mixed sample into a watch glass, dry at 85°C for 12h, and then transfer to a muffle furnace In the process, the temperature was raised to 900°C at a rate of 8°C / min, and calcined for 4h;

[0035] (2) Add the product of step (1) into 200ml deionized water, ultrasonically disperse for 1h, add 150μl of sulfuric acid, ultrasonically mix for 2h until uniform, freeze-dry, then heat up to 1200°C at a rate of 8°C / min, and calcined for 3h to obtain Phosphorus-sulfur co-doped graphene supported Mo2C material.

[0036] (3) Add the product of step (2) into deionized water, ultrasonicate for 60min, add 400mg of ammonium molybdate tetrahydrate into 20ml of deionized water, stir to d...

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Abstract

The invention discloses a phosphorus-sulfur co-doped graphene loaded Mo 2 The preparation method of C material comprises the following steps: firstly disperse graphene oxide in deionized water, add phosphoric acid and then ultrasonically mix until the solution is uniform, then freeze-dry and calcinate under nitrogen environment to obtain phosphorus-doped graphene; then phosphorus Doped graphene is ultrasonically dispersed in deionized water, after adding sulfuric acid, ultrasonically freeze-dried, and then calcined to obtain phosphorus-sulfur co-doped graphene, and then reacted with ammonium molybdate tetrahydrate, and then calcined in a hydrogen atmosphere to obtain phosphorus-sulfur co-doped graphene. Doped graphene supported Mo 2 C material. The material prepared by the method of the invention can be used for electrocatalytic nitrogen reduction, has excellent catalytic performance, and has good market prospect.

Description

technical field [0001] The invention relates to the field of nanocatalysts, specifically a phosphorus-sulfur co-doped graphene-supported Mo 2 The preparation method of C composite material. Background technique [0002] Ammonia (NH 3 ) as an important chemical substance in the world's industrial production, is widely used in the production of pharmaceuticals, synthetic fibers, fertilizers, and energy conversion processes. However, the current industrial ammonia production mainly uses the traditional Haber–Bosch method to make nitrogen (N 2 ) reduced to NH 3 . The reaction process requires pure H 2 It will consume a large amount of fossil energy as a reactant and in a high temperature and high pressure environment. Therefore, it is an urgent task to find a cleaner and more efficient ammonia production method to replace the traditional Haber–Bosch method. [0003] Electrocatalytic nitrogen reduction can synthesize ammonia at normal temperature and pressure, and the reac...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C25B11/091C25B1/27
CPCC25B1/00
Inventor 冯克君
Owner 北京时代思动科技有限公司
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